CN110237835A - A kind of titania-silica tin-graphite alkene composite photo-catalyst and preparation method thereof - Google Patents
A kind of titania-silica tin-graphite alkene composite photo-catalyst and preparation method thereof Download PDFInfo
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- CN110237835A CN110237835A CN201910507096.3A CN201910507096A CN110237835A CN 110237835 A CN110237835 A CN 110237835A CN 201910507096 A CN201910507096 A CN 201910507096A CN 110237835 A CN110237835 A CN 110237835A
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- 239000002131 composite material Substances 0.000 title claims abstract description 35
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 35
- 239000010439 graphite Substances 0.000 title claims abstract description 35
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 34
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 82
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 53
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 44
- 239000010936 titanium Substances 0.000 claims abstract description 44
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 44
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims abstract description 38
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 36
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 31
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 20
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 15
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 11
- 238000005253 cladding Methods 0.000 claims abstract description 6
- FFBHFFJDDLITSX-UHFFFAOYSA-N benzyl N-[2-hydroxy-4-(3-oxomorpholin-4-yl)phenyl]carbamate Chemical compound OC1=C(NC(=O)OCC2=CC=CC=C2)C=CC(=C1)N1CCOCC1=O FFBHFFJDDLITSX-UHFFFAOYSA-N 0.000 claims abstract description 4
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims abstract description 3
- 238000001816 cooling Methods 0.000 claims abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 25
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 24
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 claims description 24
- 239000008367 deionised water Substances 0.000 claims description 24
- 229910021641 deionized water Inorganic materials 0.000 claims description 24
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 claims description 24
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 23
- 229910001069 Ti alloy Inorganic materials 0.000 claims description 4
- HGWOWDFNMKCVLG-UHFFFAOYSA-N [O--].[O--].[Ti+4].[Ti+4] Chemical compound [O--].[O--].[Ti+4].[Ti+4] HGWOWDFNMKCVLG-UHFFFAOYSA-N 0.000 claims 1
- 239000007788 liquid Substances 0.000 claims 1
- 239000003054 catalyst Substances 0.000 abstract description 24
- 230000001699 photocatalysis Effects 0.000 abstract description 13
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 abstract description 7
- 230000015556 catabolic process Effects 0.000 abstract description 6
- 238000006731 degradation reaction Methods 0.000 abstract description 6
- 239000002086 nanomaterial Substances 0.000 abstract description 6
- 229940043267 rhodamine b Drugs 0.000 abstract description 6
- 238000002474 experimental method Methods 0.000 abstract description 5
- 239000002073 nanorod Substances 0.000 abstract description 2
- 238000010438 heat treatment Methods 0.000 description 13
- 230000003647 oxidation Effects 0.000 description 10
- 238000007254 oxidation reaction Methods 0.000 description 10
- 239000001257 hydrogen Substances 0.000 description 9
- 229910052739 hydrogen Inorganic materials 0.000 description 9
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 9
- 238000007146 photocatalysis Methods 0.000 description 9
- 238000000034 method Methods 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 2
- 241000790917 Dioxys <bee> Species 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000004043 responsiveness Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/14—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of germanium, tin or lead
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
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Abstract
The present invention relates to a kind of titania-silica tin-graphite alkene composite photo-catalysts and preparation method thereof, titanium sheet is placed under acetone and is heated, the cooling titanium sample for obtaining surface and there is carbon shell cladding titanium dioxide, titanium sample with carbon shell cladding titanium dioxide is immersed in the hydrothermal solution containing tin source, the hydro-thermal process 1~for 24 hours at 150~240 DEG C, stannic oxide graphene composite structure is generated in titanium dioxide surface, obtains titania-silica tin-graphite alkene composite photo-catalyst.The catalyst has microcosmic composite nanostructure, and surface grown the stannic oxide and Graphene nano-rod of nanostructure.The photochemical catalyst is higher to rhodamine B degradation rate in rhodamine B degradation experiment, has good visible light-responded ability and photocatalytic activity.
Description
Technical field
The present invention relates to a kind of photocatalysis technology fields, and in particular to a kind of titania-silica tin-graphite alkene is compound
Photochemical catalyst and preparation method thereof.
Background technique
Titanium dioxide has that electron hole pair potential difference is big, photochemistry corruption does not occur as a kind of semiconductor material
Erosion, soda acid patience is good, it is non-toxic, can Reusability, the characteristics such as cost is relatively low, it is latent to show huge application in photocatalysis field
Power.
According to photocatalysis technology domain requirement, photochemical catalyst need to have good visible light-responded ability and photocatalysis is living
Property.To adapt to this demand, the existing method for using the elements such as silver-doped, carbon, nitrogen is to enhance the skill of titanium deoxide catalyst
Art, but it is weaker according to TiO 2 visible light responding ability prepared by existing method, and photocatalytic activity is poor.
Summary of the invention
The present invention is in order to solve the problems in the prior art, it is compound to provide a kind of titania-silica tin-graphite alkene
Photochemical catalyst and preparation method thereof, this method by titanium dioxide surface grow stannic oxide/graphene nano structure, thus
Obtain a kind of new and effective visible light-responded property composite photo-catalyst.
To achieve the above object, the present invention adopts the following technical scheme that:
Include the following steps:
1) acetone heats: titanium sheet being placed under acetone and is heated, the cooling surface that obtains is with carbon shell cladding dioxy
Change the titanium sample of titanium；
2) hydro-thermal process: there is the titanium sample of carbon shell cladding titanium dioxide to be immersed in the water containing tin source step 1) surface
In hot solution, the hydro-thermal process 1~for 24 hours at 150~240 DEG C generates stannic oxide graphene composite junction in titanium dioxide surface
Structure obtains titania-silica tin-graphite alkene composite photo-catalyst.
Further, titanium sheet is that TA2 industrially pure titanium, TA3 industrially pure titanium, TA4 industrially pure titanium or TC4 titanium close in step 1)
Gold.
Further, the flow velocity of acetone is 0.1~50sccm in step 1).
Further, titanium sheet is placed in tube furnace and heats in step 1).
Further, the temperature heated in step 1) is 500~1000 DEG C, and the time is 30~120min.
Further, in the step 2), hydrothermal solution is by sodium hydroxide, tin tetrachloride, deionized water and anhydrous second
Alcohol is mixed to prepare, and wherein naoh concentration is 0.0001~0.8mol/L, and tin tetrachloride concentration is 0.0005~0.06mol/
L。
Further, in step 2), the volume ratio of deionized water and dehydrated alcohol is (0.5~3.5): 1.
Utilize titania-silica tin-graphite alkene composite photo-catalyst made from preparation method as described above.
Compared with prior art, the beneficial effects of the present invention are:
It is metal oxidation and crystal growth principle the present invention relates to mechanism, using acetone heating technique, acetone is used to
Carbon source is provided, the titanic oxide nanorod array that carbon shell coats can be generated in titanium and its alloy surface；The operation of graphite alkylene is carried out,
Make Surface Creation titania-silica tin-graphite alkene composite nanostructure, obtains the photocatalysis of efficient visible light-responded property
Agent.The present invention is heat-treated by hydro-thermal process, acetone atmosphere, cooperates with the titania-silica tin-graphite alkene prepared compound
Structure, including the titanium dioxide being securely grown on titanium sample, the rodlike graphene being grown on titanium dioxide, and be distributed in
Stannic oxide around graphene.Graphene and titanium dioxide it is compound, increase the contact area of photocatalytic degradation reaction, and
It is improved carrier mobility, and then promotes the photocatalysis performance of material；Utilize stannic oxide and titanium dioxide energy band position
The difference set and the internal electric field formed, further increase the transport efficiency of carrier, while reducing the compound several of electronics and hole
Rate is tested by photocatalytic degradation capability, and composite photo-catalyst of the present invention improves 4 times compared to the catalytic efficiency of pure titinium dioxide
Left and right.
Further, the present invention is by control acetone flow velocity, heating temperature etc., the nano titania that can be coated to carbon shell
Stick length, carbon thickness of the shell are regulated and controled, to prepare the photochemical catalyst with different function.
Gained catalyst of the invention has microcosmic composite nanostructure, and surface grown the stannic oxide and stone of nanostructure
Black alkene nanometer rods, titania-silica tin-graphite alkene composite catalyst structure prepared by the present invention promote electric charge transfer speed
Rate, to improve the visible light-responded performance and photocatalytic activity of photochemical catalyst.Present invention process is simple, low in cost, and
Photochemical catalyst is environmental-friendly, is easily recycled, which is expected to be widely applied in photocatalysis.The photochemical catalyst is in sieve
It is higher to rhodamine B degradation rate in red bright B degradation experiment, there is good visible light-responded ability and photocatalytic activity.It is surveying
It tries to be up to 80% to rhodamine B degradation rate in photocatalysis performance experiment.
Detailed description of the invention
Fig. 1 is the titania-silica tin-graphite alkene photochemical catalyst of efficient visible light responsiveness prepared by the present invention
Structural schematic diagram.
Specific embodiment
The present invention is described in detail with reference to the accompanying drawing.
A kind of preparation method of titania-silica tin-graphite alkene composite photo-catalyst of the invention, according to the following steps
It carries out:
1) acetone heats: the titanium sheet polished smooth is placed in tube furnace, is heated under acetone, air-cooled
To sample；Acetone flow velocity is 0.1~50sccm, and the temperature of diamond heating is 500~1000 DEG C, heating time is 30~
120min；Wherein, titanium sample is TA2, TA3, TA4 or TC4 titanium alloy.
2) hydro-thermal process: hydrothermal solution is injected in hydrothermal reaction kettle, the air-cooled obtained sample of step 1) is placed in hydro-thermal
In solution, the hydro-thermal process 1~for 24 hours at 150~240 DEG C generates stannic oxide graphene composite structure in titania surface, obtains
To the titania-silica tin-graphite alkene photochemical catalyst of efficient visible light-responded property.
Wherein hydrothermal solution is to be mixed to prepare sodium hydroxide, tin tetrachloride, deionized water and dehydrated alcohol；Wherein hydrogen-oxygen
Change na concn is 0.0001~0.8mol/L, and tin tetrachloride concentration is 0.0005~0.06mol/L.Deionized water and dehydrated alcohol
Volume ratio be (0.5~3.5): 1.
It is below specific embodiments of the present invention.
Embodiment 1
1) acetone heats: the titanium sheet polished smooth being placed in tube furnace, is heated under acetone；Acetone flow velocity is
10sccm, tubular type furnace temperature are 600 DEG C, heating time 40min；Wherein, titanium sample is TA2.
2) hydro-thermal process: hydrothermal solution is injected in hydrothermal reaction kettle, the air-cooled obtained sample of step 1) is placed in hydro-thermal
In solution, the hydro-thermal process 10h at 160 DEG C generates stannic oxide graphene composite structure in titania surface, obtains efficient
The titania-silica tin-graphite alkene photochemical catalyst of visible light-responded property.
Wherein hydrothermal solution is to be mixed to prepare sodium hydroxide, tin tetrachloride, deionized water and dehydrated alcohol；Wherein, hydrogen
Oxidation na concn is 0.0005mol/L, and tin tetrachloride concentration is 0.0005mol/L, the volume ratio of deionized water and dehydrated alcohol
For 1:1；
Embodiment 2
1) acetone heats: the titanium sheet polished smooth being placed in tube furnace, is heated under acetone；Acetone flow velocity is
20sccm, tubular type furnace temperature are 700 DEG C, heating time 60min；Wherein, titanium sample is TA3.
2) hydro-thermal process: hydrothermal solution is injected in hydrothermal reaction kettle, the air-cooled obtained sample of step 1) is placed in hydro-thermal
In solution, the hydro-thermal process 12h at 170 DEG C generates stannic oxide graphene composite structure in titania surface, obtains efficient
The titania-silica tin-graphite alkene photochemical catalyst of visible light-responded property.
Wherein hydrothermal solution is to be mixed to prepare sodium hydroxide, tin tetrachloride, deionized water and dehydrated alcohol；Wherein, hydrogen
Oxidation na concn is 0.3mol/L, and tin tetrachloride concentration is 0.025mol/L, and the volume ratio of deionized water and dehydrated alcohol is
1.5:1。
Embodiment 3
1) acetone heats: the titanium sheet polished smooth being placed in tube furnace, is heated under acetone；Acetone flow velocity is
40sccm, tubular type furnace temperature are 800 DEG C, heating time 60min；Wherein, titanium sample is TA4.
2) hydro-thermal process: hydrothermal solution is injected in hydrothermal reaction kettle, the air-cooled obtained sample of step 1) is placed in hydro-thermal
In solution, the hydro-thermal process 16h at 190 DEG C generates stannic oxide graphene composite structure in titania surface, obtains efficient
The titania-silica tin-graphite alkene photochemical catalyst of visible light-responded property.
Wherein hydrothermal solution is to be mixed to prepare sodium hydroxide, tin tetrachloride, deionized water and dehydrated alcohol；Wherein, hydrogen
Oxidation na concn is 0.45mol/L, and tin tetrachloride concentration is 0.035mol/L, and the volume ratio of deionized water and dehydrated alcohol is
2.5:1。
Embodiment 4
1) acetone heats: the titanium sheet polished smooth being placed in tube furnace, is heated under acetone；Acetone flow velocity is
20sccm, tubular type furnace temperature are 800 DEG C, heating time 120min；Wherein, titanium sample is TC4 titanium alloy.
2) hydro-thermal process: hydrothermal solution is injected in hydrothermal reaction kettle, the air-cooled obtained sample of step 1) is placed in hydro-thermal
In solution, the hydro-thermal process 18h at 220 DEG C generates stannic oxide graphene composite structure in titania surface, obtains efficient
The titania-silica tin-graphite alkene photochemical catalyst of visible light-responded property.
Wherein hydrothermal solution is to be mixed to prepare sodium hydroxide, tin tetrachloride, deionized water and dehydrated alcohol；Wherein, hydrogen
Oxidation na concn is 0.5mol/L, and tin tetrachloride concentration is 0.04mol/L, and the volume ratio of deionized water and dehydrated alcohol is 3:1.
Embodiment 5
1) acetone heats: the titanium sheet polished smooth being placed in tube furnace, is heated under acetone；Acetone flow velocity is
30sccm, tubular type furnace temperature are 700 DEG C, heating time 60min；Wherein, titanium sample is TA2.
2) hydro-thermal process: hydrothermal solution is injected in hydrothermal reaction kettle, the air-cooled obtained sample of step 1) is placed in hydro-thermal
In solution, hydro-thermal process for 24 hours, generates stannic oxide graphene composite structure in titania surface, obtains efficient at 150 DEG C
The titania-silica tin-graphite alkene photochemical catalyst of visible light-responded property.
Wherein hydrothermal solution is to be mixed to prepare sodium hydroxide, tin tetrachloride, deionized water and dehydrated alcohol；Wherein, hydrogen
Oxidation na concn is 0.0005mol/L, and tin tetrachloride concentration is 0.05mol/L, and the volume ratio of deionized water and dehydrated alcohol is
3.5:1；
Embodiment 6
1) acetone heats: the titanium sheet polished smooth being placed in tube furnace, acetone flow velocity is heated under acetone is
40sccm, tubular type furnace temperature are 900 DEG C, heating time 120min；Wherein, titanium sample is TA4.
2) hydro-thermal process: hydrothermal solution is injected in hydrothermal reaction kettle, the air-cooled obtained sample of step 1) is placed in hydro-thermal
In solution, the hydro-thermal process 1h at 240 DEG C generates stannic oxide graphene composite structure in titania surface, obtains efficient
The titania-silica tin-graphite alkene photochemical catalyst of visible light-responded property.
Wherein hydrothermal solution is to be mixed to prepare sodium hydroxide, tin tetrachloride, deionized water and dehydrated alcohol；Wherein, hydrogen
Oxidation na concn is 0.001mol/L, and tin tetrachloride concentration is 0.06mol/L, and the volume ratio of deionized water and dehydrated alcohol is
0.5:1；
Embodiment 7
1) acetone heats: the titanium sheet polished smooth being placed in tube furnace, is heated under acetone；Acetone flow velocity is
10sccm, tubular type furnace temperature are 900 DEG C, heating time 30min；Wherein, titanium sample is TA2.
2) hydro-thermal process: hydrothermal solution is injected in hydrothermal reaction kettle, the air-cooled obtained sample of step 1) is placed in hydro-thermal
In solution, the hydro-thermal process 7h at 210 DEG C generates stannic oxide graphene composite structure in titania surface, obtains efficient
The titania-silica tin-graphite alkene photochemical catalyst of visible light-responded property.
Wherein hydrothermal solution is to be mixed to prepare sodium hydroxide, tin tetrachloride, deionized water and dehydrated alcohol；Wherein, hydrogen
Oxidation na concn is 0.8mol/L, and tin tetrachloride concentration is 0.0005mol/L, and the volume ratio of deionized water and dehydrated alcohol is 1:
1；
Embodiment 8
1) acetone heats: the titanium sheet polished smooth being placed in tube furnace, is heated under acetone；Acetone flow velocity is
10sccm, tubular type furnace temperature are 900 DEG C, heating time 50min；Wherein, titanium sample is TA4.
2) hydro-thermal process: hydrothermal solution is injected in hydrothermal reaction kettle, the air-cooled obtained sample of step 1) is placed in hydro-thermal
In solution, the hydro-thermal process 5h at 200 DEG C generates stannic oxide graphene composite structure in titania surface, obtains efficient
The titania-silica tin-graphite alkene photochemical catalyst of visible light-responded property.
Wherein hydrothermal solution is to be mixed to prepare sodium hydroxide, tin tetrachloride, deionized water and dehydrated alcohol；Wherein, hydrogen
Oxidation na concn is 0.6mol/L, and tin tetrachloride concentration is 0.03mol/L, and the volume ratio of deionized water and dehydrated alcohol is 2:1；
Embodiment 9
1) acetone heats: the titanium sheet polished smooth being placed in tube furnace, is heated under acetone；Acetone flow velocity is
50sccm, tubular type furnace temperature are 900 DEG C, heating time 120min；Wherein, titanium sample is TC4 titanium alloy.
2) hydro-thermal process: hydrothermal solution is injected in hydrothermal reaction kettle, the air-cooled obtained sample of step 1) is placed in hydro-thermal
In solution, the hydro-thermal process 20h at 150 DEG C generates stannic oxide graphene composite structure in titania surface, obtains efficient
The titania-silica tin-graphite alkene photochemical catalyst of visible light-responded property.
Wherein hydrothermal solution is to be mixed to prepare sodium hydroxide, tin tetrachloride, deionized water and dehydrated alcohol；Wherein, hydrogen
Oxidation na concn is 0.05mol/L, and tin tetrachloride concentration is 0.02mol/L, and the volume ratio of deionized water and dehydrated alcohol is
2.5:1。
Referring to Fig. 1, the titania-silica tin-graphite alkene light of efficient visible light-responded property prepared by the present invention is urged
Agent includes the titanium dioxide 2 being securely grown on titanium sample 1, the rodlike graphene 3, Yi Jifen being grown on titanium dioxide 2
Stannic oxide 4 of the cloth around graphene.
When the present invention carries out photocatalysis performance test, used instrument is Shanghai than the BL-GHXII type that bright instrument produces,
Reagent to be degraded is rhodamine liquor (5ml/g), and light source is 350W xenon lamp, rhodamine B degradation experiment is carried out, by experiment
Rhodamine B drops in the measurement of front and back solution absorbance, the available titania-silica tin-graphite alkene photochemical catalyst of comparing calculation
Solution rate is up to 80%.
Claims (8)
1. a kind of preparation method of titania-silica tin-graphite alkene composite photo-catalyst, which is characterized in that including as follows
Step:
1) acetone heats: titanium sheet being placed under acetone and is heated, the cooling surface that obtains is with carbon shell cladding titanium dioxide
Titanium sample；
2) hydro-thermal process: step 1) surface is had the titanium sample of carbon shell cladding titanium dioxide, and to be immersed in the hydro-thermal containing tin source molten
In liquid, the hydro-thermal process 1~for 24 hours at 150~240 DEG C generates stannic oxide graphene composite structure in titanium dioxide surface, obtains
To titania-silica tin-graphite alkene composite photo-catalyst.
2. a kind of preparation method of titania-silica tin-graphite alkene composite photo-catalyst according to claim 1,
It is characterized in that, titanium sheet is TA2 industrially pure titanium, TA3 industrially pure titanium, TA4 industrially pure titanium or TC4 titanium alloy in step 1).
3. a kind of preparation method of titania-silica tin-graphite alkene composite photo-catalyst according to claim 1,
It is characterized in that, the flow velocity of acetone is 0.1~50sccm in step 1).
4. a kind of preparation method of titania-silica tin-graphite alkene composite photo-catalyst according to claim 1,
It is characterized in that, titanium sheet is placed in tube furnace and heats in step 1).
5. a kind of preparation method of titania-silica tin-graphite alkene composite photo-catalyst according to claim 1,
It is characterized in that, the temperature heated in step 1) is 500~1000 DEG C, the time is 30~120min.
6. a kind of preparation method of titania-silica tin-graphite alkene composite photo-catalyst according to claim 1,
It is characterized in that, hydrothermal solution is to mix sodium hydroxide, tin tetrachloride, deionized water with dehydrated alcohol in the step 2)
It is made, wherein naoh concentration is 0.0001~0.8mol/L, and tin tetrachloride concentration is 0.0005~0.06mol/L.
7. a kind of preparation method of titania-silica tin-graphite alkene composite photo-catalyst according to claim 6,
It is characterized in that, the volume ratio of deionized water and dehydrated alcohol is (0.5~3.5): 1 in step 2).
8. utilizing titania-silica tin-graphite alkene composite photo-catalyst made from preparation method described in claim 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910507096.3A CN110237835B (en) | 2019-06-12 | 2019-06-12 | Titanium dioxide-tin dioxide-graphene composite photocatalyst and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910507096.3A CN110237835B (en) | 2019-06-12 | 2019-06-12 | Titanium dioxide-tin dioxide-graphene composite photocatalyst and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN110237835A true CN110237835A (en) | 2019-09-17 |
| CN110237835B CN110237835B (en) | 2020-06-19 |
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| CN112169784A (en) * | 2020-09-23 | 2021-01-05 | 宁波石墨烯创新中心有限公司 | Titanium dioxide/graphene/carbon composite material and preparation method and application thereof |
| CN116393153A (en) * | 2023-03-20 | 2023-07-07 | 广东墨睿科技有限公司 | Graphene-nitrogen doped titanium dioxide composite material and preparation method and application thereof |
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